Magnesium turnings (5 g, i.e. 0.2 g-atom), which had been washed with absolute alcohol and dry ether, dry ether (100 ml), and a crystal of iodine were introduced into a 500-ml three-necked round-bottomed flask fitted with mercury-sealed stirrer, dropping funnel, and reflux condenser protected by a calcium chloride tube. A solution of 32 g (0.26 mole) of freshly distilled propyl bromide in 100 ml of dry ether was added dropwise from the dropping funnel (Note 1). The addition required 2–2.5 hours, and the reaction mixture was then boiled in a water bath until the magnesium had dissolved completely (90 minutes). The contents of the flask were cooled with ice and salt and stirred continuously for one hour while a solution of 18.2 g (0.19 mole) of freshly distilled 2-furaldehyde (Note 2) in 100 ml of dry ether was added. The mixture was then boiled in a water bath for 1–1.5 hours.
KeywordsAmmonium Chloride Heterocyclic Compound Reflux Condenser Seal Tube Ether Layer
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